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EP0509759B1 - Recovery of abrasive grit with a nitric acid-containing medium. - Google Patents

Recovery of abrasive grit with a nitric acid-containing medium. Download PDF

Info

Publication number
EP0509759B1
EP0509759B1 EP92303338A EP92303338A EP0509759B1 EP 0509759 B1 EP0509759 B1 EP 0509759B1 EP 92303338 A EP92303338 A EP 92303338A EP 92303338 A EP92303338 A EP 92303338A EP 0509759 B1 EP0509759 B1 EP 0509759B1
Authority
EP
European Patent Office
Prior art keywords
container
nitric acid
abrasive grit
mixture
acid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP92303338A
Other languages
German (de)
French (fr)
Other versions
EP0509759A1 (en
Inventor
Joanne Fredrica Schlimmer
Bengt Allan Karlsson
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
De Beers Industrial Diamond Division Pty Ltd
Original Assignee
De Beers Industrial Diamond Division Pty Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by De Beers Industrial Diamond Division Pty Ltd filed Critical De Beers Industrial Diamond Division Pty Ltd
Publication of EP0509759A1 publication Critical patent/EP0509759A1/en
Application granted granted Critical
Publication of EP0509759B1 publication Critical patent/EP0509759B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/065—Nitric acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D9/00—Nitrates of sodium, potassium or alkali metals in general
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/28—Acidic compositions for etching iron group metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • This invention relates to a process which uses an acidic medium containing nitric acid.
  • the essential feature of the process of the invention is that it is carried out in a suitable oxidising atmosphere in a closed container.
  • This has the effect of oxidising nitrogen oxide gases, particularly nitrous oxide, produced by the process.
  • Nitrous oxide is oxidised to nitric oxide which dissolves in the water of the acidic medium. In this manner nitric acid is regenerated. Thus, the consumption of nitric acid is substantially reduced. Further, the necessity to neutralise the effluent is also substantially reduced.
  • the chemical reactions which take place are:
  • the container in which the reaction takes place is closed in the sense that it is closed or sealed to atmosphere.
  • Such containers e.g. pressure cylinders are well known in the art and any such container may be used. During the process gases are produced and so the pressure within the container will tend to rise to an equilibrium state which is above atmospheric pressure.
  • the oxidising atmosphere will have an oxygen content of at least 40 percent by volume.
  • the source of the oxygen may be oxygen in gaseous form or a material such as a peroxide which will release oxygen.
  • the oxidising atmosphere will typically be oxygen-enriched air or oxygen.
  • the process will generally be carried out on a batch basis although it can also be carried out on a continuous basis.
  • the acidic medium will preferably be, or contain, a mixture of sulphuric and nitric acids.
  • the source of the nitric acid may be nitric acid itself or a suitable nitrate such as sodium nitrate. In this latter case, sodium nitrate may be mixed with concentrated sulphuric acid and then diluted, if desired, with water.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • ing And Chemical Polishing (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Processing Of Solid Wastes (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A process such as a leaching, etching or pickling process which uses an aqueous acidic medium containing nitric acid is improved by carrying out the process in the presence of an oxidising atmosphere in a closed container.

Description

    BACKGROUND OF THE INVENTION
  • This invention relates to a process which uses an acidic medium containing nitric acid.
  • There are many processes which use acidic mediums containing nitric acid, i.e. nitrate containing acids. Such processes are, for example, leaching, etching and pickling. Acidic effluents are produced by such processes and these effluents have to be neutralised. This requires the use of substantial quantities of alkali. Also, the consumption of nitric acid is high. A further problem with these processes is the emission of nitrogen oxide gases which give rise to environmental problems.
    • SUMMARY OF THE INVENTION
  • The invention is as set forth in Claim 1.
    • DESCRIPTION OF EMBODIMENTS
  • The essential feature of the process of the invention is that it is carried out in a suitable oxidising atmosphere in a closed container. This has the effect of oxidising nitrogen oxide gases, particularly nitrous oxide, produced by the process. Nitrous oxide is oxidised to nitric oxide which dissolves in the water of the acidic medium. In this manner nitric acid is regenerated. Thus, the consumption of nitric acid is substantially reduced. Further, the necessity to neutralise the effluent is also substantially reduced. The chemical reactions which take place are:
    Figure imgb0001
    Figure imgb0002
    Figure imgb0003
  • The container in which the reaction takes place is closed in the sense that it is closed or sealed to atmosphere. Such containers, e.g. pressure cylinders are well known in the art and any such container may be used. During the process gases are produced and so the pressure within the container will tend to rise to an equilibrium state which is above atmospheric pressure.
  • Generally, the oxidising atmosphere will have an oxygen content of at least 40 percent by volume. The source of the oxygen may be oxygen in gaseous form or a material such as a peroxide which will release oxygen. The oxidising atmosphere will typically be oxygen-enriched air or oxygen.
  • The process will generally be carried out on a batch basis although it can also be carried out on a continuous basis.
  • The acidic medium will preferably be, or contain, a mixture of sulphuric and nitric acids. The source of the nitric acid may be nitric acid itself or a suitable nitrate such as sodium nitrate. In this latter case, sodium nitrate may be mixed with concentrated sulphuric acid and then diluted, if desired, with water.
  • A process, as described above, was used to recover diamond grit from a reaction capsule in which the metal body was cobalt. This process was compared with a conventional recovery process carried out in a vessel open to atmosphere and the results obtained are set out below.
    Figure imgb0004
  • The advantages of the process of the invention over that of the prior art can be seen from the above table. First, the consumption of nitric acid is substantially reduced. Second, the total liquid effluent is reduced resulting in less consumption of neutralising alkali. Third, the nitric fume emission is substantially reduced improving the environmental friendliness of the leaching process. Finally, the recovery of the diamond grit by the process of the invention was as good as that obtained with the prior art method.
  • The process described above was repeated using 0,3 bar oxygen pressure. The dissolution of the metal took somewhat longer, but the remaining advantages over the prior art process were the same.

Claims (5)

1. A process of recovering abrasive grit from a reaction capsule containing the grit dispersed in a metal body, including the steps of crushing the capsule and the metal body, mixing the crushed mass with a nitrate or an acidic medium containing nitric acid, charging a container with the mixture, agitating the mixture, adding an acid other than nitric acid to the container, replacing the gas in the container with an oxidising atmosphere, adding water to the mixture in the container, sealing the container to atmosphere, pressurising the container to a pressure above atmospheric with an oxidising atmosphere, allowing the acidic medium to dissolve the metal in the container and release the abrasive grit, bringing the contents of the container to ambient pressure, removing liquid from the container and recovering the abrasive grit.
2. A process according to Claim 1 wherein the oxidising atmosphere has an oxygen content of at least 40 percent by volume.
3. A process according to Claim 1 or Claim 2 wherein the oxidising atmosphere is oxygen-enriched air or oxygen.
4. A process according to any one of the preceding Claims wherein the acidic medium contains a mixture of sulphuric and nitric acids.
5. A process according to any one of Claims 1 to 4 wherein the other acid is sulphuric acid.
EP92303338A 1991-04-15 1992-04-14 Recovery of abrasive grit with a nitric acid-containing medium. Expired - Lifetime EP0509759B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ZA912785 1991-04-15
ZA912785 1991-04-15

Publications (2)

Publication Number Publication Date
EP0509759A1 EP0509759A1 (en) 1992-10-21
EP0509759B1 true EP0509759B1 (en) 1994-06-22

Family

ID=25580628

Family Applications (1)

Application Number Title Priority Date Filing Date
EP92303338A Expired - Lifetime EP0509759B1 (en) 1991-04-15 1992-04-14 Recovery of abrasive grit with a nitric acid-containing medium.

Country Status (9)

Country Link
US (1) US5324496A (en)
EP (1) EP0509759B1 (en)
JP (1) JPH05106064A (en)
KR (1) KR0166980B1 (en)
AT (1) ATE107712T1 (en)
CA (1) CA2065964A1 (en)
DE (1) DE69200202T2 (en)
IE (1) IE65475B1 (en)
ZA (1) ZA922589B (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4291886B2 (en) * 1994-12-05 2009-07-08 住友電気工業株式会社 Low defect diamond single crystal and synthesis method thereof
US5578222A (en) * 1995-12-20 1996-11-26 Saint-Gobain/Norton Industrial Ceramics Corp. Reclamation of abrasive grain
JPH09217132A (en) * 1996-02-13 1997-08-19 Santoku Kinzoku Kogyo Kk Method for recovering useful elements from rare earth-iron alloys
WO1998008585A1 (en) * 1996-08-26 1998-03-05 Geochem Technologies, Inc. Leaching of metal chalcogenide (sulfide-type) minerals with oxidizing and chelating agents
KR20070092219A (en) 2004-12-06 2007-09-12 코닌클리케 필립스 일렉트로닉스 엔.브이. Etching Solution and Additives
DE102015113589A1 (en) * 2015-08-17 2017-02-23 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Method and device for processing a HNO3-containing liquid process agent

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2805940A (en) * 1954-08-20 1957-09-10 Bennedsen Hans Oluf Process for extracting cobalt and nickel from their ores
US2947611A (en) * 1958-01-06 1960-08-02 Gen Electric Diamond synthesis
GB905282A (en) * 1960-08-03 1962-09-05 Kestner Evaporator And Enginee A method of pickling metal parts in nitric acid
NL128759C (en) * 1965-11-13
US3965239A (en) * 1973-11-16 1976-06-22 International Ore Technology, Inc. Recovery of nitric acid soluble transition metals from sulfur and iron containing ores of the same
FR2259913B1 (en) * 1974-02-05 1976-11-26 Nickel Le
US3945865A (en) * 1974-07-22 1976-03-23 Dart Environment And Services Company Metal dissolution process
DE2601017C3 (en) * 1976-01-13 1981-05-21 Didier-Werke Ag, 6200 Wiesbaden Process for reducing pollutant emissions when pickling metals and equipment for carrying out the process
US4084961A (en) * 1976-09-10 1978-04-18 Sunshine Mining Company Treatment of metal bearing mineral material
US4224380A (en) * 1978-03-28 1980-09-23 General Electric Company Temperature resistant abrasive compact and method for making same
US4670051A (en) * 1985-03-19 1987-06-02 Hydrochem Developments Ltd. Oxidation process for releasing metal values in which nitric acid is regenerated in situ
US4931068A (en) * 1988-08-29 1990-06-05 Exxon Research And Engineering Company Method for fabricating fracture-resistant diamond and diamond composite articles

Also Published As

Publication number Publication date
CA2065964A1 (en) 1992-10-16
JPH05106064A (en) 1993-04-27
KR920019669A (en) 1992-11-19
IE65475B1 (en) 1995-11-01
ZA922589B (en) 1992-12-30
DE69200202T2 (en) 1994-11-10
ATE107712T1 (en) 1994-07-15
EP0509759A1 (en) 1992-10-21
IE921192A1 (en) 1992-10-21
DE69200202D1 (en) 1994-07-28
US5324496A (en) 1994-06-28
KR0166980B1 (en) 1999-01-15

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